HRID1383951

反应详情

EQUATION

反应方程式

HRID 1383951 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 4-[4-[2-(2-hydroxyethylthio)ethoxy]phenyl]-1,1,1-trifluoro-2-butanone (1.20 g, 3.72 mmol), 4,4′-dimethylbenzhydrol (0.95 g, 4.47 mmol) and p-toluenesulfonic acid (0.035 g) in toluene (20 ml) was heated under reflux for 15 min. The cooled reaction mixture was diluted with ethyl acetate, washed with saturated sodium bicarbonate, brine and dried (magnesium sulfate). Evaporation of the solvent in vacuo and chromatography of the residue on silica gel (elution with a gradient of ethyl acetate 20-40% in hexane) gave 1.81 g (94%) of the title material as an oil.

WORKUP

后处理

  1. temperatureunder reflux for 15 min
  2. customThe cooled reaction mixture
  3. washwashed with saturated sodium bicarbonate, brine
  4. dry with materialdried (magnesium sulfate)
  5. customEvaporation of the solvent in vacuo and chromatography of the residue on silica gel (
  6. washelution with a gradient of ethyl acetate 20-40% in hexane)